Publication date: 15th December 2025
Mo2C is a promising and efficient catalyst in alkaline media for electrochemical hydrogen evolution reaction (HER), attributed to improved charge transfer characteristics.[1] However, under reactions conditions of alkaline HER, this catalyst undergoes dynamic reconstruction and dissolution to generate MoOx species at the electrode-electrolyte interface.[2] The factors influencing the generation of these species, and the contribution of these species toward electrocatalytic activity demands an in-depth investigation. To enable this study, we designed Mo2C, and Mo/Mo2C heterostructures with varying Mo content, and used electrochemical techniques, in situ spectro-electrochemical experiments, and several post-stability ex situ characterisation methods to ascertain the dynamics of formation of these species, and deduce their contribution toward electrocatalytic activity. Synchrotron based in situ X-ray absorption spectroscopy (XAS) and Raman analyses reveal that the catalysts undergo chemical oxidation in alkaline medium and structural reconstruction under electrochemical conditions. Post stability X-ray absorption spectroscopy analysis, it is found that Mo2C in situ generates MoOx species with a local coordination environment resembling that of MoO2, which correlates with enhanced HER activity (117 mV overpotential @ 10 mAcm-2). Furthermore, the in situ formed (and regenerable) active species from reconstructed Mo2C consist of defective MoOx species which bestows the catalyst with high activity. Moreover, in Mo/Mo2C, a major fraction of Mo forms water-soluble MoO42− (molybdate) species which subsequently leads to diminished HER activity. The combined experimental and density functional theory (DFT) calculations have inferred the vital role of reconstruction of Mo2C toward improved HER activity. Our findings reveal key aspects of surface reconstruction and local coordination environment of Mo2C systems informing the mechanism-driven development of advanced HER electrocatalyst.
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